CN102499238B - Method for preparing sustained-release insecticide microcapsule by using supercritical fluid technology - Google Patents
Method for preparing sustained-release insecticide microcapsule by using supercritical fluid technology Download PDFInfo
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- CN102499238B CN102499238B CN 201110380469 CN201110380469A CN102499238B CN 102499238 B CN102499238 B CN 102499238B CN 201110380469 CN201110380469 CN 201110380469 CN 201110380469 A CN201110380469 A CN 201110380469A CN 102499238 B CN102499238 B CN 102499238B
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- release
- microcapsule
- supercritical fluid
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000003094 microcapsule Substances 0.000 title claims abstract description 16
- 239000002917 insecticide Substances 0.000 title claims abstract description 11
- 239000012530 fluid Substances 0.000 title claims abstract description 7
- 238000005516 engineering process Methods 0.000 title abstract description 4
- 238000013268 sustained release Methods 0.000 title abstract description 4
- 239000012730 sustained-release form Substances 0.000 title abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 7
- 229960000892 attapulgite Drugs 0.000 claims abstract description 6
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 6
- 229920002678 cellulose Polymers 0.000 claims abstract description 5
- 239000001913 cellulose Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 235000011089 carbon dioxide Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000000575 pesticide Substances 0.000 claims description 5
- 235000016068 Berberis vulgaris Nutrition 0.000 claims description 4
- 241000335053 Beta vulgaris Species 0.000 claims description 4
- 235000007516 Chrysanthemum Nutrition 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 3
- -1 ester amine Chemical class 0.000 claims description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 244000189548 Chrysanthemum x morifolium Species 0.000 claims 1
- 239000004615 ingredient Substances 0.000 abstract description 4
- 230000000749 insecticidal effect Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 abstract 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 229960003237 betaine Drugs 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 239000004531 microgranule Substances 0.000 abstract 1
- 241000255925 Diptera Species 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 5
- 241000723353 Chrysanthemum Species 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 241000256113 Culicidae Species 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000003197 gene knockdown Methods 0.000 description 2
- 241000238876 Acari Species 0.000 description 1
- 241000256186 Anopheles <genus> Species 0.000 description 1
- 235000018958 Gardenia augusta Nutrition 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000257226 Muscidae Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a method for preparing a sustained-release insecticide microcapsule by using a supercritical fluid technology. A composition prepared with the method comprises ingredients, such as cellulose, attapulgite, essence, a betaine ampholytic surface active agent and the like. The method comprises the following steps of: compounding the above ingredients; and further evenly covering particles with a supercritical impact micro-granule wrapping method. With the method, the agglomeration tendency which easily appears when the common means are adopted is lightened so as to improve the evenness of the microcapsule. Meanwhile, the method also has the universal advantages of the traditional supercritical wrapping method. The composition prepared with the method has a good insecticidal effect and an obvious sustained-release effect.
Description
Technical field
The present invention relates to a kind of method for preparing Domestic controlled-release insecticidal composition, relate in particular to a kind of method for preparing the slow-release pesticide microcapsules with supercritical fluid technique.The composition of the method preparation is suitable for being used for by Sprayable the desinsection of indoor and closed environment, and it can slowly discharge insecticidal active ingredient, the lasting effectiveness of killing that keeps for common pathogenic insects of family such as mosquito, fly, dirt mites.
Background technology
The chrysanthemum ester type compound can be used for mosquito control, and has higher insecticidal activity, to be widely known by the people.But the existing various liquid that wipes out the flies and mosquitoes, spray during use in indoor in the market, and drug volatilization is fast, effective kill pests, but because medicine discharges rapidly, duration of efficacy is very short, needs to spray constantly, makes troubles to the user.Disclose a kind of long-acting concentrated incecticide for soaking and painting use in Chinese patent application 95111196, but that this product exists is poisonous, have peculiar smell, effective time still not long, and uses inconvenience.Therefore people need a kind of nontoxic, free from extraneous odour, the insecticide that spraying once just can be permanently effective.Therefore the improvement for the insecticide preparation method just seems particularly important.
Summary of the invention
Purpose of the present invention just is for the deficiencies in the prior art, and a kind of method for preparing the slow-release pesticide microcapsules with supercritical fluid technique is provided.
The objective of the invention is to realize by following measures:
A kind of method for preparing the slow-release pesticide microcapsules with supercritical fluid technique, it comprises the following steps:
1) with cellulose, attapulgite, essence, beet alkali ampholytic surface active agent by 85 parts: 100 parts: 0.5 part: the weight ratio of 0.1 part joins in the acetone soln of 0.1% (wt) chrysanthemum ester amine of 500 parts, obtains mixed liquor 40 ℃～50 ℃ lower mixing and stirring;
2) this mixed liquor is placed in autoclave, adds the carbonic acid gas after boosting by high-pressure diaphragm pump in the autoclave, heating up and stirring forms suspension;
3) this suspension is clashed into by coaxial a pair of nozzle ejection staggered relatively, the coating microcapsule particle of separating out separates by gas-solid separator with carbonic acid gas and namely gets insecticide slow-release microcapsule product.
Cellulose wherein can be CMC or hydroxyethylcellulose.
Beet alkali ampholytic surface active agent wherein can be CTFA or 11 carbonamido acetic acid betains.
As mentioned above, the present invention is by using advanced overcritical shock particle encapsulation method, further realized the even coating of particle, alleviated the reunion tendency that easily occurs in the conventional means, thereby improved the uniformity of microcapsules, also had the general advantage of existing overcritical method for coating simultaneously.
Simultaneously for coordinating above-mentioned preparation technology's demand, the product that processability meets the requirements, in the present invention, used attapulgite as the capsule core component on the one hand, take full advantage of the load capacity that its larger specific surface brings, make effective insecticide ingredient be carried on its surface and inner, not only saved expensive insecticide consumption but also improved the distributional pattern of insecticide, increase itself and extraneous contacting, be conducive to strengthen effect and the sustained release of Pesticidal combination.
On the other hand, the present invention has used amphoteric surfactant to attapulgite modified, promote the load of insecticide ingredient in its surface and gap by improving its oleophylic performance, and improved to a certain extent the even distribution of clad material, extend the time that desinsection effect keeps, improved simultaneously its wide spectrum adaptability for the different solvents medium.
Embodiment
Embodiment 1
The preparation of product A: 1) with CMC, attapulgite, cream jasmin france, CTFA by 85 parts: 100 parts: 0.5 part: the weight ratio of 0.1 part joins in the acetone soln of 0.1% (wt) chrysanthemum ester amine of 500 parts, obtains mixed liquor 40 ℃～50 ℃ lower mixing and stirring;
2) this mixed liquor is placed in autoclave, adds the carbonic acid gas after boosting by high-pressure diaphragm pump in the autoclave, be warming up to and form supercriticality and stir and form suspension;
3) this suspension is clashed into by coaxial a pair of nozzle ejection staggered relatively, the coating microcapsule particle of separating out separates by gas-solid separator with carbonic acid gas, collects the microcapsule particle that separates and namely gets insecticide slow-release microcapsule product A.
Embodiment 2
The preparation of product B: use hydroxyethylcellulose to replace CMC, use 11 carbonamido acetic acid betains to replace CTFA, repeat the preparation method of embodiment 1, make product B.
Embodiment 3
Properties of product tests: product A and B are added respectively water, and evenly to be hybridly prepared into the atomized liquid of 0.1% (wt) standby, 30 houseflies alive, 20 anopheles alive are put into respectively each airtight chamber, spray into respectively the atomized liquid of product A and B on the tank wall with spray method, spray value is 5ml.The beginning timing and regularly observed and recorded knock down number of elements after 24 hours, remove the mosquitos and flies in case, chamber is placed after 72 hours and is put into respectively the mosquitos and flies of similar number again, the beginning timing and regularly observed and recorded knock down number of elements after 24 hours.Carry out simultaneously the blank test.The results are shown in down.
Claims (1)
1. method for preparing the slow-release pesticide microcapsules with supercritical fluid technique, it comprises the following steps:
1) with cellulose, attapulgite, essence, beet alkali ampholytic surface active agent by 85 parts: 100 parts: 0.5 part: the weight ratio of 0.1 part joins in the acetone soln of 0.1% (wt) chrysanthemum ester amine of 500 parts, obtains mixed liquor 40 ℃～50 ℃ lower mixing and stirring;
2) this mixed liquor is placed in autoclave, adds the carbonic acid gas after boosting by high-pressure diaphragm pump in the autoclave, heating up and stirring forms suspension;
3) this suspension is clashed into by coaxial a pair of nozzle ejection staggered relatively, the coating microcapsule particle of separating out separates by gas-solid separator with carbonic acid gas and namely gets insecticide slow-release microcapsule product,
Wherein, described cellulose is CMC or hydroxyethylcellulose, and described beet alkali ampholytic surface active agent is CTFA or 11 carbonamido acetic acid betains.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110380469 CN102499238B (en) | 2011-11-25 | 2011-11-25 | Method for preparing sustained-release insecticide microcapsule by using supercritical fluid technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110380469 CN102499238B (en) | 2011-11-25 | 2011-11-25 | Method for preparing sustained-release insecticide microcapsule by using supercritical fluid technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102499238A CN102499238A (en) | 2012-06-20 |
| CN102499238B true CN102499238B (en) | 2013-06-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201110380469 Expired - Fee Related CN102499238B (en) | 2011-11-25 | 2011-11-25 | Method for preparing sustained-release insecticide microcapsule by using supercritical fluid technology |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109483420A (en) * | 2018-12-05 | 2019-03-19 | 郑州磨料磨具磨削研究所有限公司 | A kind of Ultra-fine ceramic abrasive tool supercritical fluid method for mixing |
| CN110117906A (en) * | 2019-05-08 | 2019-08-13 | 安徽省翰先纺织科技有限公司 | Printed fabric production technology |
| CN110283012A (en) * | 2019-06-13 | 2019-09-27 | 徐悦阳 | A kind of Pesticidal and sterilizing organic fertilizer and preparation method thereof |
| CN115005202A (en) * | 2022-07-11 | 2022-09-06 | 南开大学 | Surfactant-induced pesticide intercalation attapulgite nano hybrid and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792157A (en) * | 2005-12-30 | 2006-06-28 | 山东农业大学 | High performance cypermethrin micro-capsule emulsion |
| CN101648955A (en) * | 2009-09-04 | 2010-02-17 | 北京化工大学常州先进材料研究院 | Method for extracting chlorophyll from spirulina by using supercritical fluid |
| CN101716198A (en) * | 2010-01-25 | 2010-06-02 | 淮阴工学院 | Method for preparing total ginkgo flavone glycosides slow-release capsules by applying attapulgite |
| EP2263455A1 (en) * | 2008-04-17 | 2010-12-22 | Ishihara Sangyo Kaisha, Ltd. | Harmful organism control composition, and method for control of harmful organisms |
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2011
- 2011-11-25 CN CN 201110380469 patent/CN102499238B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792157A (en) * | 2005-12-30 | 2006-06-28 | 山东农业大学 | High performance cypermethrin micro-capsule emulsion |
| EP2263455A1 (en) * | 2008-04-17 | 2010-12-22 | Ishihara Sangyo Kaisha, Ltd. | Harmful organism control composition, and method for control of harmful organisms |
| CN101648955A (en) * | 2009-09-04 | 2010-02-17 | 北京化工大学常州先进材料研究院 | Method for extracting chlorophyll from spirulina by using supercritical fluid |
| CN101716198A (en) * | 2010-01-25 | 2010-06-02 | 淮阴工学院 | Method for preparing total ginkgo flavone glycosides slow-release capsules by applying attapulgite |
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| CN102499238A (en) | 2012-06-20 |
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